Preservation of liquid foods



24, 1945. R LEE PRESERVATION OF LIQ UID FQODS Filed Jui s, 1940 m R T mm v m G w L T D m T E0 O A Fm F W@ PL 6 SEMI-PERMEABLE S E M R B M E M ment, and I Fig. 5 is'a fragmentary sectional elevation of PatentedeA pr. 24.19 45 UNlTED [STATE s PATENT orrlca PRESERVATION OF FOODS Royal Lee, Milwaukee, Wis., assignor to Lee Foundation for Nutritional Research, Milwaukee, Wis a corporation of Wisconsin,

Application July 3, 1940, Serial No. 343,841

5 Claims. (0!. 99-155) The present invention relates to the preserva- 1 tion of perishable liquid substances, more particularly liquid foods. such as fruit and vegetable juices. I n I An object of the invention is to provide a method of concentrating and-sterilizing food juices and the like without materially altering their.

natural characteristics, such as flavor, nutrient value and vitamin content.

Another object'of the invention is to provide I an improved method of producing a sterilized dry substance from a juice.

A further object ls'to provide improved apparatus for effecting the preservation of the liquid substances.

The invention further consists in the several features hereinafter described and claimed.

a In the accompanying drawing, L

Fig. 1 is a diagrammatic view of a vacuum type evaporating apparatus for concentrating juice and for removing-a sterilizing liquid therefrom, parts of the apparatus being shown in section; Fig. 2 is a diagrammatic view of an apparatus for sterilizing juice by the application of ultrasonic waves, parts of the apparatus being shown in section; I

Fig. 3 is a diagrammatic side elevation apparatus for dialyzing the juice;

Fig. 4 is an elevation of a dialyzer frame eleof an the dialymr.

to remove this material as the flavor and food valuesof orange juiceand other fruit juices are present to a considerableextent in the suspended materials. It is desirable to conduct the freezing and centrifuging inan oxygen-free atmosphere, such as of nitrogen or carbon dioxide.

The concentrated juice is then sterilized in one or more of various ways hereinafter set forth which will avoid heating the juice to pasteurizing temperature and thereby minimize deterioration of the juice. In some instances, the juice is further concentrated to a dry substance, as hereinafter described.

One method of sterilizing involves the use of certain volatile organic solvents such as chloroform and toluene, or mixtures-thereof, the solvents being suitably dispersed through the juice,

' as by shaking or emulsifying. The action of. these solvents is to dissolve :the cell walls of microorganisms. Only a relatively small quantity of these solvents is required, say 1 to 5% of the juice by volume, and slightly in excess of the amount required for solution of the soluble materialscf V the juice'.. The solvent is subsequently removed from the juice, as by the use of a vacuum still or evaporator, 'the solution being kept below pasteurizing temperature. Preferably the solvent is recovered for reuse. In certain cases some of the water content of the juice will also be removed along with-the solvent, and can be separated 'therefrom'in various ways, as by fractional distillation. In order to facilitate dispersion of the The invention isapplicable to the preservation of a wide variety of perishable liquid substances and more particularly fruit and vegetable juices,

for example, orange juice, grape juice, carrot juice, sugar-cane juice, and sorghum juice.

By way of example, the invention will be ex-.

plained in connection with the treatment of fruit juice such as orange juice.

, It is first desirable to deaerate the juice, as by subjecting the juice to a vacuum. Thisremoves the dissolved gases, especially oxygen, which might otherwise cause deterioration of the juice, such as loss of flavor and color and destruction of vitamins.

The juice is then partially dehydrated, preferably'by freezing. Most of the water is thus segregated as ice, and most of the pulp and other suspended solids are trapped in the ice. The ice 7 mass-is crushed and is centrifuged to remove the concentrated juice. This treatment avoids filtra- Juice.

Another method of sterilizing consists in desterilizingsolvent through the juice, the solvent may first be dissolved in a small quantity of another solvent, preferably ethyl alcohol, freely v miscible in water.

stroying the micro-organisms by'subjecting the concentrated juice to mechanical wave energy. This will produce cavitation" or mechanical destruction of the micro organisms.

. Still another method of sterilization consistsin treating the juice with high frequency electrical energy, preferably in the' range of frequencies tion difliculties' which would otherwise be encoun- I tered as the colloidal material of the juice. would tend toclog a filter. Moreover, it is not desirable corresponding to 1 to 30 meters wave length. This treatment can be effected by passing thejuice between plate electrodes fora short period, such The proportions are not as one to five minutes. The energy is applied either in a band of frequencies or by varying the frequency during the period of treatment, in order to insure destruction of various molds and other microorganisms having different lethal frequen-,

conduits 2a and the cells 21 'are serially connected by conduits 30. The incoming raw Juice,

eithernormal or concentrated. enters a cell 26 at --one end of the series, while sterllewater. is adcies. The juice is cold during this treatment, or

at least below the pasteurizing temperature.

A further method of sterilization consists in di'- alyzing or filtering the juice. This can be done only in the case of a juice such as sugar-cane juice, where the colloidal constituents are relatively unimportant and their loss can .be' tolerated. l

The concentrated sterile iuice produced by the various treatments'above described may be bottled or marketed as such, or it may be passed through a spray drier to provide a dry powder, as when a raw. sugar is desired from cane Juice. The drying mitted to the cell 21 at the other end of the series. The raw juice flows through'the cells 26 in succession and the soluble constituents thereof pass through the membranes into the intervening cells 21, whereas any micro-organisms present are prevented from passing into the latter cells. The

" waste of the Juice is finally discharged from the is preferably eilectedin an atmosphere free of oxygen. In the case of fruit juices, the powder form obviates the "transportation of water, and insures good keeping qualities. The fruit juice powder is useful inmaking confections, or it may be reconstituted into a liquid by the addition of water. If desired, thepowder .may be pressed into tablets or pellets.

Spray dryin of liquids has heretoforeinvolved I the application of suflicient heat to sterilize'the product. When sterilization is accomplished with volatile'solvents, they are easily removed in the spraying process'without other steps and at a temperature below the pasteurizing tempera- In Fig. l of the drawing there is shown a vacuum evaporating apparatus for removing the sterilizing solvent from the juice, and for further concentrating the juice. This apparatus includes a corrugated tube In through which the sterile juice solution flows downwardly in a'fllm along the inner walls of the tube, the rate of flow into the tube being controlled by a valve II. The

tube has a jacket l2' through which water or other heating medium is passed in an upward direction. Thetemperature of the water is below pasteurizing temperature, but is sutliciently high,

, say about 125 to produce evaporation of the solvent at'a reasonably rapid rate. Some of the water content of the juice will also be evaporated. The tube H) has its bottom or discharge end connected to a vessel l3 which receives the sterile concentrated juice. A conduit It extends from the vessel It to a condenser l6 from which the condensate flows into a vessel l6. A conduit l1 leads from the vessel l6 to any suitable vacuum pump; not ;shown.

Anapparatus for sterilizing the juice' by the application of mechanical wave energy is shown in Fig. 2. A conduit Ill admits the liquid at high pressure and high velocity into a valve chamber l6 havingtw. outlet ports and 2| communicating with respective branch conduits 22 and 23 which merge into a single outlet conduit 26, the latter discharging into a receiving tank 25 in which a suitable pressure is maintained. A rotary valve 26 mounted in the chamber 16 rotates at high speed and admits the liquid alternately into the branch conduits 22 and 23, setting up mechanical waves in the branch conduits to sterilize the juice therein.

Th dialyzing apparatus shown in Figs. 3 to 5 '7 serves to sterilize and filter thejuice. This apparatus includes a series of dialyzing cells 26 and 21 separated by semi-permeable membrane 26, the cells 26 and 21 being arranged in alternate relation. The cells 26 are serially connected by last cell 26. The incoming sterile water flows through the-cells 21 in oounterflow relation to the ,cells 26 and gradually acquires the soluble constituents of the raw juice, the purified liquid or juice'being finally'discharged from the last cell 21.

The cells are formed by a pack of parallel loopshaped' frames 3| and the membranes 26, the

. assembly being'completed by end plates 32 which are secured in position by clamping bolts 63.

Each frame vis provided at opposite ends with bolt-receiving notches 34 which serve to retain vthe frames in alignment. The frames are formed branes. The liquid in each cell flows from one end r the frame to the other, and the liquid in adjacent cells flows in opposite directions. A

suiiicient number of cells is provided to minimize los of soluble materials in the waste liquid.

In cases where the juice is reduced to a dried substance, such as powdered or granular mass,

it is sometimes desirable to sterilize the dried substance instead of sterilizing the Juice, In such cases the juice is dried, as by spray drying or other process, at a temperature below the pasteurizingtemperature. The dried substance is then mixed with a small quantity of a volatile liquid sterilizing agent, such as one or more of the agents above mentioned, a suflicient amount of the liquid being added to dampen or saturate the dried substance. Preferably, a sterilizing liquid is used which willnot appreciably dissolve the dried substance. The sterilizing liquid is then evaporated from the resulting product, as in a rotary drier, at a temperature below the pasteurizing temperature, the product being agitated in the drier. Theliquid may also be removed by subjecting the product to a vacuum,

and supplying heat to facilitate evaporation, the temperature, however, being well below the pasteurizing point. Instead-of using a liquid sterilizing agent, a gaseous sterilizing agent may be used, such as formaldehyde and methyl formate.

vPreferably, the dried substance is subjected the vacuum before treatment with these'sterilizing agents in order to insure thorough penetration. In some instances it is desirable to aeratethe sterilized dried substance in order to remove all traces of the liquid or gaseous sterilizing agent.

While certain ways of carrying out the invention have been described above, it will be understood that changes and modifications may be made without departing fromthe spirit and.

scope of the invention as expressed'by the appended claims. a

emetic ing solvent, and then simultaneously eveporeting the solvent from the sterilised Juice and drying the juice. 2. The method of preserving a food juice which consists in dispensing therein a volatile orgenic .sterllilinI solvent, and then spray-drying the sterilised juice at e tempers-tum below the. peeteurising temperature of the Juice.

"3; The method of preserving a food Juice which -eonslsuindispening-therein enorgenic sterilisthe mg solvent, end then subjecting sterilised mm In. min ng ot lzhe ebow're numbered patent frequir-ingoorrectionne :l'ollow sgPege 1, secand column, "solvent"- reed --'-so1vent. ethyl alcohol. us ede16 line 9,-"c1e1m gea rets;

' Letters" 7 Potent should.

3 the solvent juice to e drying operetionto remove end to convert the Juice to a dry substance.

7 consists in therein an organic sterilizor money;

n3? b mdi i 4. .The' method 01 preservinge food Juice which consists in dispersing therein en' organic sterilizing solvent which is relatively insoluble in water. and then evenoratin'g the solvent from the sterilized juice and drying the Juice.

5. The method 0! preserving a. food juice which consists in edding thereto an organic sterilizing solvent selected from a group consisting of chlomiorm end toluene end dissolved in en organic solvent freely miscible with water, end'then removing the solvents from the sterilized "Juice and drying the Juice.

in the .Patent Office m conform lto them-score or tl m Signed and sealed this 5 5?? u 19,45?

(Seal) Leslie Frazer v noting Commissioner of Patents In eqne instances, or sterilli'zing' -e page 5, firet' colmnn, i-em "dispersin and that the said is correction therein that the some emetic ing solvent, and then simultaneously eveporeting the solvent from the sterilised Juice and drying the juice. 2. The method of preserving a food juice which consists in dispensing therein a volatile orgenic .sterllilinI solvent, and then spray-drying the sterilised juice at e tempers-tum below the. peeteurising temperature of the Juice.

"3; The method of preserving a food Juice which -eonslsuindispening-therein enorgenic sterilisthe mg solvent, end then subjecting sterilised mm In. min ng ot lzhe ebow're numbered patent frequir-ingoorrectionne :l'ollow sgPege 1, secand column, "solvent"- reed --'-so1vent. ethyl alcohol. us ede16 line 9,-"c1e1m gea rets;

' Letters" 7 Potent should.

3 the solvent juice to e drying operetionto remove end to convert the Juice to a dry substance.

7 consists in therein an organic sterilizor money;

n3? b mdi i 4. .The' method 01 preservinge food Juice which consists in dispersing therein en' organic sterilizing solvent which is relatively insoluble in water. and then evenoratin'g the solvent from the sterilized juice and drying the Juice.

5. The method 0! preserving a. food juice which consists in edding thereto an organic sterilizing solvent selected from a group consisting of chlomiorm end toluene end dissolved in en organic solvent freely miscible with water, end'then removing the solvents from the sterilized "Juice and drying the Juice.

in the .Patent Office m conform lto them-score or tl m Signed and sealed this 5 5?? u 19,45?

(Seal) Leslie Frazer v noting Commissioner of Patents In eqne instances, or sterilli'zing' -e page 5, firet' colmnn, i-em "dispersin and that the said is correction therein that the some 

